#------------------------------------------------------------------------------
#$Date: 2017-08-31 16:48:46 +0300 (Thu, 31 Aug 2017) $
#$Revision: 200038 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/08/2020871.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2020871
loop_
_publ_author_name
'Kelley, Annette'
'Nalla, Sowjanya'
'Bond, Marcus R.'
_publ_section_title
;
 The square-planar to flattened-tetrahedral CuX42−(X= Cl, Br)
 structural phase transition in 1,2,6-trimethylpyridinium salts
;
_journal_coeditor_code           OG5072
_journal_issue                   1
_journal_name_full
'Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials'
_journal_page_first              48
_journal_page_last               60
_journal_paper_doi               10.1107/S205252061402664X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_moiety         '2(C8 H12 N), Br4 Cu'
_chemical_formula_sum            'C16 H24 Br4 Cu N2'
_chemical_formula_weight         627.55
_chemical_name_systematic
;
bis(1,2,6-trimethylpyridinium) tetrabromidocuprate(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 113.631(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0879(12)
_cell_length_b                   9.4953(10)
_cell_length_c                   8.7957(9)
_cell_measurement_reflns_used    1207
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     1001.41(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8979
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         4.98
_exptl_absorpt_coefficient_mu    9.071
_exptl_absorpt_correction_T_max  0.341
_exptl_absorpt_correction_T_min  0.140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             606
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.125
_refine_diff_density_max         1.807
_refine_diff_density_min         -1.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1097P)²+4.1327P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1729
_refine_ls_wR_factor_ref         0.183
_reflns_number_gt                1013
_reflns_number_total             1212
_reflns_threshold_expression     >2sigma(I)
_iucr_refine_instructions_details
;
TITL bond103 in C 2/m
CELL  0.71073  13.0879   9.4953   8.7957   90.000  113.631   90.000
ZERR     4.00   0.0012   0.0010   0.0009    0.000    0.006    0.000
LATT   7
SYMM  - X,   Y, - Z
SFAC  C    H    N    CU   BR
UNIT  32   48   4    2    8
MERG   2
EQIV $1 x,-y,z
BIND C4 C3_$1
FMAP   2
PLAN   25
ACTA
BOND   $H
LIST   4
L.S.   4
WGHT    0.109700    4.132700
FVAR       0.38088
CU1   4    0.000000    0.000000    0.000000    10.25000    0.02854    0.02819 =
         0.02473    0.00000    0.01348    0.00000
BR1   5    0.062964    0.000000    0.295405    10.50000    0.03637    0.02867 =
         0.02539    0.00000    0.01366    0.00000
BR2   5    0.000000    0.257730    0.000000    10.50000    0.03864    0.02795 =
         0.02574    0.00000    0.01474    0.00000
N1    3    0.171544    0.500000    0.702715    10.50000    0.02387    0.03486 =
         0.03607    0.00000    0.01255    0.00000
C11   1    0.208003    0.500000    0.886777    10.50000    0.03406    0.04219 =
         0.02612    0.00000    0.01124    0.00000
AFIX 123
H11A  2    0.214191    0.595296    0.925934    10.25000   -1.50000
H11B  2    0.279121    0.454211    0.937559    10.25000   -1.50000
H11C  2    0.154138    0.450492    0.915182    10.25000   -1.50000
H11D  2    0.217442    0.404704    0.926516    10.25000   -1.50000
H11E  2    0.152512    0.545789    0.914891    10.25000   -1.50000
H11F  2    0.277495    0.549508    0.937268    10.25000   -1.50000
AFIX   0
C2    1    0.157680    0.375371    0.621734    11.00000    0.02610    0.03077 =
         0.03459    0.00189    0.01462    0.00007
C21   1    0.174317    0.239299    0.715610    11.00000    0.03764    0.02909 =
         0.03129    0.00314    0.01823   -0.00234
AFIX 137
H21A  2    0.250719    0.231758    0.792776    11.00000   -1.50000
H21B  2    0.156162    0.161845    0.639141    11.00000   -1.50000
H21C  2    0.126705    0.237294    0.774934    11.00000   -1.50000
AFIX   0
C3    1    0.125983    0.374437    0.452898    11.00000    0.03029    0.03264 =
         0.02902   -0.00568    0.01267   -0.00470
AFIX  43
H3    2    0.115969    0.289449    0.396174    11.00000   -1.20000
AFIX   0
C4    1    0.109082    0.500000    0.367911    10.50000    0.03272    0.03156 =
         0.03077    0.00000    0.01480    0.00000
AFIX  43
H4    2    0.086281    0.500000    0.253250    10.50000   -1.20000
HKLF    4
REM  bond103 in C 2/m
REM R1 =  0.0598 for   1013 Fo > 4sig(Fo)  and  0.0715 for all   1212 data
REM     62 parameters refined using      0 restraints
END
;
_cod_data_source_file            og5072sup1_Br100K.cif
_cod_data_source_block           Br100K
_cod_original_cell_volume        1001.41(17)
_cod_database_code               2020871
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.0000 0.0000 0.0000 0.0263(4) Uani d S 1 4 . .
Br Br1 0.06296(8) 0.0000 0.29540(11) 0.0297(4) Uani d S 1 2 . .
Br Br2 0.0000 0.25773(10) 0.0000 0.0302(4) Uani d S 1 2 . .
N N1 0.1715(7) 0.5000 0.7027(12) 0.0314(18) Uani d S 1 2 . .
C C11 0.2080(9) 0.5000 0.8868(12) 0.034(2) Uani d S 1 2 . .
H H11A 0.2142 0.5953 0.9259 0.052 Uiso calc PR 0.25 1 . .
H H11B 0.2791 0.4542 0.9376 0.052 Uiso calc PR 0.25 1 . .
H H11C 0.1541 0.4505 0.9152 0.052 Uiso calc PR 0.25 1 . .
H H11D 0.2174 0.4047 0.9265 0.052 Uiso calc PR 0.25 1 . .
H H11E 0.1525 0.5458 0.9149 0.052 Uiso calc PR 0.25 1 . .
H H11F 0.2775 0.5495 0.9373 0.052 Uiso calc PR 0.25 1 . .
C C2 0.1577(6) 0.3754(7) 0.6217(9) 0.0297(15) Uani d . 1 1 . .
C C21 0.1743(6) 0.2393(7) 0.7156(9) 0.0313(15) Uani d . 1 1 . .
H H21A 0.2507 0.2318 0.7928 0.047 Uiso calc R 1 1 . .
H H21B 0.1562 0.1618 0.6391 0.047 Uiso calc R 1 1 . .
H H21C 0.1267 0.2373 0.7749 0.047 Uiso calc R 1 1 . .
C C3 0.1260(6) 0.3744(7) 0.4529(9) 0.0304(15) Uani d . 1 1 . .
H H3 0.1160 0.2894 0.3962 0.036 Uiso calc R 1 1 . .
C C4 0.1091(9) 0.5000 0.3679(13) 0.031(2) Uani d S 1 2 . .
H H4 0.0863 0.5000 0.2532 0.037 Uiso calc SR 1 2 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cu1 0.0285(8) 0.0282(8) 0.0247(8) 0.000 0.0135(7) 0.000
Br1 0.0364(6) 0.0287(5) 0.0254(5) 0.000 0.0137(4) 0.000
Br2 0.0386(6) 0.0279(5) 0.0257(5) 0.000 0.0147(4) 0.000
N1 0.024(4) 0.035(4) 0.036(5) 0.000 0.013(3) 0.000
C11 0.034(5) 0.042(6) 0.026(5) 0.000 0.011(4) 0.000
C2 0.026(3) 0.031(4) 0.035(4) 0.000(3) 0.015(3) 0.002(3)
C21 0.038(4) 0.029(3) 0.031(4) -0.002(3) 0.018(3) 0.003(3)
C3 0.030(3) 0.033(4) 0.029(3) -0.005(3) 0.013(3) -0.006(3)
C4 0.033(5) 0.032(5) 0.031(5) 0.000 0.015(4) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
Br2 Cu1 Br1 5_656 . 90.000(10)
C2 N1 C2 . 6 121.6(9)
C2 N1 C11 . . 119.1(5)
N1 C11 H11A . . 109.5
N1 C11 H11B . . 109.5
H11A C11 H11B . . 109.5
N1 C11 H11C . . 109.5
H11A C11 H11C . . 109.5
H11B C11 H11C . . 109.5
N1 C11 H11D . . 109.5
H11A C11 H11D . . 141.1
H11B C11 H11D . . 56.3
H11C C11 H11D . . 56.3
N1 C11 H11E . . 109.5
H11A C11 H11E . . 56.3
H11B C11 H11E . . 141.1
H11C C11 H11E . . 56.3
H11D C11 H11E . . 109.5
N1 C11 H11F . . 109.5
H11A C11 H11F . . 56.3
H11B C11 H11F . . 56.3
H11C C11 H11F . . 141.1
H11D C11 H11F . . 109.5
H11E C11 H11F . . 109.5
N1 C2 C3 . . 119.5(7)
N1 C2 C21 . . 120.2(7)
C3 C2 C21 . . 120.3(6)
C2 C21 H21A . . 109.5
C2 C21 H21B . . 109.5
H21A C21 H21B . . 109.5
C2 C21 H21C . . 109.5
H21A C21 H21C . . 109.5
H21B C21 H21C . . 109.5
C2 C3 C4 . . 119.7(7)
C2 C3 H3 . . 120.2
C4 C3 H3 . . 120.2
C3 C4 C3 6 . 119.9(10)
C3 C4 H4 . . 120
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cu1 Br1 . 2.3903(10)
Cu1 Br2 . 2.4472(10)
N1 C2 . 1.355(8)
N1 C11 . 1.493(14)
C11 H11A . 0.96
C11 H11B . 0.96
C11 H11C . 0.96
C11 H11D . 0.96
C11 H11E . 0.96
C11 H11F . 0.96
C2 C3 . 1.372(11)
C2 C21 . 1.501(9)
C21 H21A . 0.96
C21 H21B . 0.96
C21 H21C . 0.96
C3 C4 . 1.377(9)
C3 H3 . 0.93
C4 H4 . 0.93

_cod_database_fobs_code 2020871
